[关键词]
[摘要]
目的 采用高效液相色谱-电喷雾检测器(HPLC-CAD)法同时测定小建中片中氧化芍药苷、芍药内酯苷、芍药苷、甘草苷、异甘草苷、桂皮酸、桂皮醛、甘草酸。方法 采用Agilent Zorbax Eclipse XDB C18色谱柱(250 mm×4.6 mm,5μm);流动相:90%甲醇-10 mmol/L甲酸铵(甲酸调pH 3.5),梯度洗脱;体积流量:0.9 mL/min;柱温:30℃;进样量:20μL;CAD雾化器温度:35℃,采集频率为10 Hz,过滤常数为5.0。结果 氧化芍药苷、芍药内酯苷、芍药苷、甘草苷、异甘草苷、桂皮酸、桂皮醛、甘草酸的线性范围分别为1.02~20.40、12.08~241.60、13.99~279.80、3.05~61.00、1.10~22.00、0.24~4.80、1.20~24.00、1.12~22.40μg/mL;平均加样回收率分别为99.4%、97.1%、98.2%、98.9%、99.3%、97.5%、99.1%、98.8%,RSD值分别为1.8%、0.9%、1.8%、2.0%、2.3%、1.6%、2.0%、1.6%。结论 该方法同时测定小建中片中8个活性成分,实现多指标成分质量控制,为小建中片的质量标准规范化研究提供参考。
[Key word]
[Abstract]
Objective To develop HPLC-CAD method for simultaneous determination of oxypaeoniflora, albiflorin, paeoniflorin, liquiritin, isoliquiritin, cinnamic acid, cinnamaldehyde, and glycyrrhizic acid in Xiaojianzhong Tablets. Methods The chromatographic separation was performed on Agilent Agilent Zorbax Eclipse XDB C18 column (250 mm×4.6 mm, 5 μm) with 90% methanol - 10 mmol/L ammonium acetate (formic acid tone pH 3.5) as the mobile phase for gradient elution. The flow rate was 0.9 mL/min, the column temperature was set at 30 ℃, and injection volume was 20 μL. The nebulization temperature of detector was set at 35 ℃, the acquisition frequency was 10 Hz, and the filtration constant was 5.0. Results The linear ranges of eight components were 1.02 — 20.40、12.08 — 241.60、13.99 — 279.80、3.05 — 61.00、1.10 — 22.00、0.24 — 4.80、1.20 — 24.00、1.12 — 22.40 μg/mL, respectively. The average recoveries were 99.4%, 97.1%, 98.2%, 98.9%, 99.3%, 97.5%, 99.1%, and 98.8%, and the RSD values were 1.8%, 0.9%, 1.8%, 2.0%, 2.3%, 1.6%, 2.0%, and 1.6%, respectively. Conclusion The method can simultaneously determine 8 active ingredients in Xiaojianzhong Tablets, and realizes the quality control of multi-index component, which provides a reference for the standardization research of Xiaojianzhong Tablets.
[中图分类号]
R286.02
[基金项目]